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US5376450A Expired / Lapsed US ⏱️ 0.0 years remaining

Low surface acid intercalated graphite and method

Assignee: Graftech Inc
•
Filing: 1992-09-30
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Granted: 1994-12-27
•
Expires: 2012-09-30
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Abstract

Abstract Particles of intercalated graphite are formed by treating graphite particles with an intercalant and contacting the graphite particles with an organic molecule having C8-C30 carbon atoms and a polar end functional group.

Inventors

  • 👤 Ronald A. Greinke
  • 👤 Richard I. Bretz

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-31 03:52
CPC Classifications
C; C04; C04B; C04B35/00; C04B35/622; C04B35/626; C01; C01B; C01B32/00; C01B32/20; C01B32/21; C01B32/22; Y; Y10; Y10T; Y10T428/00; Y10T428/29; Y10T428/2982; Y10T428/2991; Y10T428/30

Claims Analysis

Total Claims: 9
Claim 1
Independent Claim 206 words
A process for manufacturing particles of intercalated graphite having no greater than about 1.5% average titratable surface acid by weight comprising the steps of (a) treating particles of graphite with an intercalant comprising a solution of one or more members selected from the group consisting of nitric acid sulfuric acid, potassium chlorate, chromic acid, potassium permanganate, potassium chromate, potassium dichromate, perchloric acid, hydrogen peroxide, iodic acid, periodic acid, ferric chloride and other metal halides to provide intercalated particles of graphite having edge separated layer planes with acid intercalant therebetween in graphene galleries; (b) washing said intercalated particles of graphite with water to substantially close the edges of said layer planes and remove exposed surface acid therefrom; (c) drying said washed particles; and (d) contacting said particles of graphite before said drying step with an effective amount of an agent composed of an organic molecule having a long chain hydrocarbon group with at least eight carbon atoms and a polar functional end group such that at least a minimum concentration of 0.35 pph of said agent is present on said particles during said drying step so that said closed edges of said layer planes remain substantially closed and the exposure of acid intercalant therebetween is essentially avoided.
Claim 2
Dependent Claim 206 words
A process for manufacturing particles of intercalated graphite having no greater than about 1.5% average titratable surface acid by weight comprising the steps of (a) treating particles of graphite with an intercalant comprising a solution of one or more members selected from the group consisting of nitric acid sulfuric acid, potassium chlorate, chromic acid, potassium permanganate, potassium chromate, potassium dichromate, perchloric acid, hydrogen peroxide, iodic acid, periodic acid, ferric chloride and other metal halides to provide intercalated particles of graphite having edge separated layer planes with acid intercalant therebetween in graphene galleries; (b) washing said intercalated particles of graphite with water to substantially close the edges of said layer planes and remove exposed surface acid therefrom; (c) drying said washed particles; and (d) contacting said particles of graphite before said drying step with an effective amount of an agent composed of an organic molecule having a long chain hydrocarbon group with at least eight carbon atoms and a polar functional end group such that at least a minimum concentration of 0.35 pph of said agent is present on said particles during said drying step so that said closed edges of said layer planes remain substantially closed and the exposure of acid intercalant therebetween is essentially avoided.
Claim 3
Dependent Claim 46 words
A process as defined in claim 1 wherein said agent is a surfactant with a molecular structure having a hydrophobic long chain hydrocarbon group of between C 10 -C 30 carbon atoms and a polar functional end group which can be anionic, cationic, zwitterionic or nonionic.
Claim 4
Dependent Claim 83 words
A process as defined in claim 2 wherein said surfactant has the generic formula R(X) where R is the hydrocarbon group and X is selected from the group consisting of --COOZ, --SO 3 Z, --NH 2 , --NH + 3 , --N + H 2 CH 2 --COO - , --N(CH 3 ) 2 CH 2 COO - , ##STR2## and --OH, where Z is H, an alkyl group having 1 to 6 carbon atoms, an alkali metal or NH + 4 .
Claim 5
Dependent Claim 22 words
A process as defined in claim 3 wherein said surfactant is insoluble in water and is added to the washed graphite particles.
Claim 6
Dependent Claim 21 words
A process as defined in claim 4 wherein the minimum concentration of said surfactant is between 0.35 pph and 1.0 pph.
Claim 7
Dependent Claim 117 words
Intercalated particles of graphite having an average titratable surface acid concentration of no greater than about 1.5% by weight and a specific worm volume of greater than about 150 cc/g when exfoliated, wherein said particles are formed by the process of treating particles of graphite with an intercalant, washing said treated particles with water, drying said graphite particles and contacting said particles of graphite, before said drying step with an effective amount of an organic molecule agent having a long chain hydrocarbon group with at least eight carbon atoms and a polar functional end group such that at least a minimum concentration of 0.35 pph of said agent is present on said particles during said drying step.
Claim 8
Dependent Claim 117 words
Intercalated particles of graphite having an average titratable surface acid concentration of no greater than about 1.5% by weight and a specific worm volume of greater than about 150 cc/g when exfoliated, wherein said particles are formed by the process of treating particles of graphite with an intercalant, washing said treated particles with water, drying said graphite particles and contacting said particles of graphite, before said drying step with an effective amount of an organic molecule agent having a long chain hydrocarbon group with at least eight carbon atoms and a polar functional end group such that at least a minimum concentration of 0.35 pph of said agent is present on said particles during said drying step.
Claim 9
Dependent Claim 46 words
Intercalated particles of graphite as defined in claim 6 wherein said organic molecule agent is a surfactant composed of a hydrophobic long chain hydrocarbon group with C 10 -C 30 carbon atoms and a polar functional end group which can be anionic, cationic, zwitterionic or nonionic.

References Cited (Backward Citations)

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USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1997-12-26 1998-06-27 1998-12-27 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 2001-12-26 2002-06-27 2002-12-27 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 2005-12-26 2006-06-27 2006-12-27 $7700.00 Window Closed / Lapsed

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